CN102220491A - Method for recovering manganese from manganese ore, manganese tailing and manganese slag through continuous pressurization and acid leaching process - Google Patents
Method for recovering manganese from manganese ore, manganese tailing and manganese slag through continuous pressurization and acid leaching process Download PDFInfo
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- CN102220491A CN102220491A CN2011101487209A CN201110148720A CN102220491A CN 102220491 A CN102220491 A CN 102220491A CN 2011101487209 A CN2011101487209 A CN 2011101487209A CN 201110148720 A CN201110148720 A CN 201110148720A CN 102220491 A CN102220491 A CN 102220491A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to a method for recovering manganese from manganese ore, manganese tailing and manganese slag through a continuous pressurization and acid leaching process, which comprises the following steps: (1) preparing manganese raw material which is the manganese ore, the manganese tailing or the manganese slag; (2) pulverizing the raw material; (3) adding water into the raw material, and uniformly mixing for getting ore slurry; (4) adding sulfuric acid into the ore slurry and adjusting for getting the acid-containing ore slurry; (5) continuously adding the acid-containing ore slurry into a leaching kettle which can be sealed, adjusting the feeding speed and ensuring the retention time of the acid-containing ore slurry in the leaching kettle; (6) continuously adding the acid-containing ore slurry into the leaching kettle, adjusting the working pressure, keeping the pressure, adjusting the working temperature, keeping the temperature and stirring; (7) discharging the ore slurry from the leaching kettle; (8) and performing liquid-solid separation to get manganese-containing leachate. The method has the benefits that the manganese, in particular to high-valence manganese in the manganese ore, the manganese tailing and the manganese slag with complex composition can be directly leached. By adopting the method, the leaching rate of the manganese is high and operation conditions are improved; and the leaching process can be operated continuously, so that the operation efficiency and the labor productivity are greatly improved. The method has the characteristics of advanced process, convenience in operation, high utilization rate of resources, high leaching rate of the manganese, short operation time, short process flow, high labor productivity and environment friendliness.
Description
Technical field
The present invention relates to a kind of method that reclaims manganese with the method for hydrometallurgy.It specifically is the continuous pressurized acid leaching method of a kind of usefulness reclaims manganese from manganese ore, manganese mine tailing and manganese slag method.
Background technology
Electrolytic metal Mn and manganese salt are important material in the national economy.Though there is the manganese resource than horn of plenty in China, based on medium and small mineral deposit, and ore grade is lower.China is maximum in the world manganese country of consumption, and manganese ore output far can not be satisfied the demand.Main industry-the Iron And Steel Industry of manganese consumption relies on a large amount of import ANOMALY IN FINE QUALITY MANGANESE DEPOSITS to produce needs to satisfy.The hydrometallurgy of manganese metal produces how to soak manganese ore with aqueous sulfuric acid, makes the manganese pass into solution in the manganese ore, again with the solution electrodeposition.Since sulfuric acid can only with the reaction of bivalent manganese mineral such as manganese carbonate ore, all must be as handle Manganse Dioxide and other high price manganese mineral with pickling process through pre-treatment, will the reduction of high price manganese being converted into bivalent manganese, could to adopt sulfuric acid to soak molten.Therefore, adopt direct leaching process to handle the manganese hydrometallurgy factory and the manganese factory of manganese ore, general all with manganese carbonate ore or mainly be the divalence manganese ore of manganese carbonate ore or mix manganese ore as raw material.In the pretreatment technology of various high price manganese, the reducing roasting technology of thermal process transforms the control difficulty owing to bivalent manganese under condition of high temperature oxidation very easily again makes, transformation efficiency is difficult to guarantee, and also there are factors such as energy consumption is big, processing charges height, in enterprise, how have been eliminated; Though pyrite+Manganse Dioxide sinter process reduction effect is better, because of the factor such as seriously polluted that has technical problem and low concentration sulphur dioxide flue gas is not seen report in industrial application as yet.Using more is the direct acid leaching processes in two ore deposits, and promptly the pyrite that adds some amount in the dioxide ore for manganese directly leaches in sulfuric acid system as reductive agent.Utilize the iron sulphide reductibility of sulphur under high acidity condition at a middle or low price, the high price manganese in the manganese oxide ore is reduced to bivalent manganese, self be oxidized to sulfuric acid or elemental sulfur simultaneously.
The existing production technique of manganese hydrometallurgy, no matter be manganese carbonate ore acidleach or the direct acid leaching process of two ore deposit methods, leaching operation process all carries out in uncovered steel basin, be subjected to restrictions such as air pressure conditions and acid mist, moisture evaporation and steam consumption are big, processing temperature generally can only be below 85 ℃, the transformation efficiency of manganese ore is not high, leaching rate is low, manganese leaching yield general 65%～70%; The operation process interruption is carried out in addition, and leaching generally needs 6～8 hours working cycle, and production efficiency is low, and operating condition is poor, and labour intensity is big.During the raw material of manganese ore hydrometallurgy enterprise of China and manganese chemical product enterprise is mainly domestic, low-grade mixing manganese ore, the manganous carbonates that adopt in the direct acid leaching process leaching ore, the manganese milltailings of a large amount of low-grade manganese oxide ores and the residue behind the leaching manganous carbonate have been stored up in production over the years more.Manganese resource not only in short supply does not obtain fine recycling, also a large amount of land occupations and cause environmental pollution.
Summary of the invention
For overcoming prior art high price manganese is needed reducing roasting, residue behind low-grade manganese oxide ore, manganese milltailings and leaching manganous carbonate reclaimed manganese efficient is low, yield is low, problem of environment pollution caused, the continuous pressurized acid leaching method of a kind of usefulness reclaims manganese from manganese ore, manganese mine tailing and manganese slag method is proposed, this method can directly be soaked the manganese in manganese ore, manganese mine tailing and the manganese slag of molten mineral composition complexity, and production efficiency height, the direct yield height of manganese, and free from environmental pollution.
Technical scheme of the present invention is: the continuous pressurized acid leaching method of a kind of usefulness reclaims the method for manganese from manganese ore, manganese mine tailing and manganese slag, the steps include:
(1) be equipped with the manganese raw material, described manganese raw material is at least a in manganese ore, manganese mine tailing or the manganese slag;
(2) raw material pulverizing, levigate;
(3) raw material adds water 300%～700%, adds reductive agent, mixes to be ore pulp;
(4) acid adjustment, adding sulfuric acid in ore pulp, to be adjusted into acid content be containing of 20g/L～200g/L of sour ore pulp;
(5) charging will contain the leaching still that the continuous adding of sour ore pulp can seal, and adjust input speed, make that to contain the residence time of sour ore pulp in leaching still be 60min～180min;
(6) leach, will contain sour ore pulp and add continuously when leaching still, in leaching still, add gas, the operating pressure that leaches still is adjusted to 0.3MPa～1.5Mpa, keep-ups pressure 95 ℃～150 ℃ of working temperatures, keep temperature, stir, extraction time is 60min～180min;
(7) discharging is discharged ore pulp from leach still;
(8) liquid-solid separation obtains containing the manganese leach liquor.
Mn in the described manganese raw material of step (1)
AlwaysThe content mass percent be 5%～60%, Mn wherein
2+Content 0%～100%, all the other are high price manganese; Described high price manganese is meant that the valency of manganese in compound is greater than 2.
The described pulverizing of step (2) is to-100 orders～+ 400 orders with raw material pulverizing.
Step (2) and (3) described raw material are to add reductive agent in the manganese raw material, and reductive agent is a pyrite, and reductive agent is crushed to-200 orders, and the mass ratio of manganese raw material and reductive agent is 100:0～50.
The described charging of step (5) is by force (forcing) pump ore pulp to be carried to leaching still.
Step (5), (6) and (7) described autoclave are that horizontal multicell high pressure leaches still, or leach stills with pipeline a plurality of vertical high pressure of connecting.
Described the keep-uping pressure of step (6) is to realize by input pressurized air in leaching still; The described maintenance temperature of step (6) is to realize by input steam in leaching still.
The speed of the described stirring of step (7) is 15～750 rev/mins.
The present invention is that the method for the continuous pressurized acid leaching of employing makes rapid, the fully leaching of manganese in the manganese raw material, the present invention adopts pressurization and improves method of temperature and strengthen reaction process, improve the speed of reaction of leaching process and the leaching yield of manganese, the present invention through test and Selection specific pressure and temperature, make leaching yield and cost reach best.For make the high price manganese can fully leach, the present invention can add pyrite as reductive agent, the ratio of reductive agent be according in the raw material high price manganese amount design.The present invention pulverizes manganese raw material and reductive agent, and the manganese in the raw material can fully be leached.Be to guarantee the pressurized acid leaching implementation of processes, leaching plant of the present invention is to adopt the leaching still that can seal, and whole acidleach process is to carry out being higher than under the state of barometric point, has improved the leaching yield of manganese, has avoided the reactant gases effusion.The present invention is the speed by control charging and discharging, finishes leaching process when raw material is moved in leaching still, thereby has realized continuous production.Raw material is the time of high pressure acidleach metallurgical reaction process the working time from opening for feed to discharge port, and equipment of the present invention mainly is that horizontal multicell high pressure leaches still, and also the placed in-line a plurality of vertical high pressure of available pipe leach still.For guarantee that leaching process carries out under high pressure and hot conditions, the present invention needs to add high pressure steam to satisfy process thermal equilibrium and to keep working temperature in leaching process; Add pressurized air with control autoclave working pressure.The present invention needs continuously stirring in leaching process, make leaching evenly, fully, through liquid-solid separation, obtains containing the manganese leach liquor, leach liquor is produced according to a conventional method manganese metal or other manganese product again.The present invention goes for various manganese raw materials, is specially adapted to high price manganese and the lower manganese raw material of grade.
The principal reaction formula that manganese leaches in manganese ore of the present invention, manganese mine tailing and the manganese slag is:
15MnO
2?+?2FeS
2?+?14H
2SO
4?＝?15MnSO
4?+?Fe
2(SO
4)
3?+?14H
2O
MnCO
3?+?H
2SO
4?＝?MnSO
4?+?CO
2?+?H
2O
The beneficial effect of the invention is: can directly leach the manganese of forming in complicated manganese ore, manganese mine tailing and the manganese slag, particularly high price manganese.Compare with existing manganese wet metallurgical leaching process, the adaptability of raw material significantly promotes and can reclaim resource from discarded manganese slag, helps improving the utilization ratio of manganese resource; Leaching operation carries out in the autoclave of sealing, control still internal pressure is higher than normal pressure, material is leached under higher temperature of reaction, strengthened reaction process, increase substantially the conversion leaching yield of speed of reaction and manganese, shortened extraction time, the soaking molten and reclaim of high efficiency realization manganese oxide ore, adopt method of the present invention to make the leaching yield height of manganese, soaking slag, to contain manganese very low; The operation calorific loss that the large quantity of moisture evaporation brings in the leaching process of in closed container, having avoided heating, avoid simultaneously the reactant gases of overflowing in the operation process and acid mist pollution environment and to operator's harm, operating condition improved; Leaching process carries out continuously, reduces the subsidiary operation time of being interrupted drill traverse significantly, and operating efficiency and labour productivity are significantly improved; Process intensification.Technology advanced person of the present invention, easy to operate, the resource utilization height, manganese leaching yield height, the activity duration is short, and technical process is short, labour productivity height, eco-friendly characteristics.
Embodiment
The method that reclaims manganese with continuous pressurized acid leaching method from manganese ore, manganese mine tailing and manganese slag provides 6 embodiment, and concrete parameter sees Table 1, and concrete steps are as follows:
(1) be equipped with manganese raw material and reductive agent,
(2) with manganese raw material and reductive agent separated pulverizing,
(3) batching, the weight ratio of each raw material: manganese raw material: reductive agent is 100: 0～50,
(4) manganese raw material and reductive agent are added water, mix and be ore pulp,
(5) acid adjustment, adding sulfuric acid in ore pulp is that acid content is containing of 20g/L～200g/L of a sour ore pulp,
(6) charging is will contain sour ore pulp continuously by force (forcing) pump to add and leach still, adjusts input speed, make ore pulp in autoclave from the residence time that is fed to discharging be 60min～180min,
(7) leach, in leaching still, add gas, the operating pressure that leaches still is adjusted to 0.3MPa～1.5Mpa,, keep leaching the constant pressure of design in the still by in leaching still, importing pressurized air; 95 ℃～150 ℃ of working temperatures are imported steam in leaching still, keep leaching the homo(io)thermism of design in the still, stir, and extraction time is to be 60min～180min the ore pulp residence time,
(8) discharging is discharged ore pulp from leach still,
(9) with the liquid-solid separation of ordinary method, obtain containing the manganese leach liquor, detect the content of manganese in the leach liquor,
(10) with ordinary method purification of leaching liquor and electrodeposition are got manganese metal.
Table 1
Claims (8)
1. one kind is reclaimed the method for manganese with continuous pressurized acid leaching method from manganese ore, manganese mine tailing and manganese slag, the steps include:
(1) be equipped with the manganese raw material, described manganese raw material is at least a in manganese ore, manganese mine tailing or the manganese slag;
(2) raw material pulverizing;
(3) raw material adds water 300%～700%, mixes to be ore pulp;
(4) acid adjustment, adding sulfuric acid in ore pulp, to be adjusted into acid content be containing of 20g/L～200g/L of sour ore pulp;
(5) charging will contain the leaching still that the continuous adding of sour ore pulp can seal, and adjust input speed, make that to contain the residence time of sour ore pulp in leaching still be 60min～180min;
(6) leach, will contain sour ore pulp and add continuously when leaching still, in leaching still, add gas, the operating pressure that leaches still is adjusted to 0.3MPa～1.5Mpa, keep-ups pressure 95 ℃～150 ℃ of working temperatures, keep temperature, stir, extraction time is 60min～180min;
(7) discharging is discharged ore pulp from leach still;
(8) liquid-solid separation obtains containing the manganese leach liquor.
2. the continuous pressurized acid leaching method of a kind of usefulness according to claim 1 reclaims the method for manganese from manganese ore, manganese mine tailing and manganese slag, it is characterized in that: Mn in the described manganese raw material of step (1)
AlwaysThe content mass percent be 5%～60%, Mn wherein
2+Content 0%～100%, all the other are high price manganese; Described high price manganese is meant that the valency of manganese in compound is greater than 2.
3. the continuous pressurized acid leaching method of a kind of usefulness according to claim 1 reclaims the method for manganese from manganese ore, manganese mine tailing and manganese slag, it is characterized in that: the described pulverizing of step (2) is to-100 orders～+ 400 orders with raw material pulverizing.
4. the continuous pressurized acid leaching method of a kind of usefulness according to claim 1 reclaims the method for manganese from manganese ore, manganese mine tailing and manganese slag, it is characterized in that: step (2) and (3) described raw material are to add reductive agent in the manganese raw material, reductive agent is a pyrite, reductive agent is crushed to-200 orders, and the mass ratio of manganese raw material and reductive agent is 100:0～50.
5. the continuous pressurized acid leaching method of a kind of usefulness according to claim 1 reclaims the method for manganese from manganese ore, manganese mine tailing and manganese slag, it is characterized in that: the described charging of step (5) is by force (forcing) pump ore pulp to be carried to leaching still.
6. the continuous pressurized acid leaching method of a kind of usefulness according to claim 1 reclaims the method for manganese from manganese ore, manganese mine tailing and manganese slag, it is characterized in that: step (5), (6) and (7) described autoclave are that horizontal multicell high pressure leaches still, or leach stills with pipeline a plurality of vertical high pressure of connecting.
7. the continuous pressurized acid leaching method of a kind of usefulness according to claim 1 reclaims the method for manganese from manganese ore, manganese mine tailing and manganese slag, it is characterized in that: described the keep-uping pressure of step (6) is to realize by input pressurized air in leaching still; The described maintenance temperature of step (6) is to realize by input steam in leaching still.
8. the continuous pressurized acid leaching method of a kind of usefulness according to claim 1 reclaims the method for manganese from manganese ore, manganese mine tailing and manganese slag, it is characterized in that: the speed of the described stirring of step (7) is 15～750 rev/mins.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101487209A CN102220491A (en) | 2011-06-03 | 2011-06-03 | Method for recovering manganese from manganese ore, manganese tailing and manganese slag through continuous pressurization and acid leaching process |
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| CN2011101487209A CN102220491A (en) | 2011-06-03 | 2011-06-03 | Method for recovering manganese from manganese ore, manganese tailing and manganese slag through continuous pressurization and acid leaching process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102605187A (en) * | 2011-10-10 | 2012-07-25 | 云南建水锰矿有限责任公司 | Method for producing manganese sulfate by manganese-rich slag through pressure leaching |
| CN102703698A (en) * | 2012-07-11 | 2012-10-03 | 昆明永瑞防腐有限公司 | Wet metallurgical method for spessartite mineral |
| CN103436696A (en) * | 2013-09-06 | 2013-12-11 | 宁夏天元锰业有限公司 | Method for preparing stock solution for electrolysis to produce metal manganese |
| CN104480314A (en) * | 2014-12-17 | 2015-04-01 | 赵阳臣 | Method for recycling waste residue in manganese industry production |
| CN106756003A (en) * | 2017-01-12 | 2017-05-31 | 江苏凯力克钴业股份有限公司 | The production method that a kind of use potential control is continuously leached |
| WO2024108266A1 (en) * | 2022-11-25 | 2024-05-30 | Element 25 Limited | Process for the recovery of manganese |
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| CN101157481A (en) * | 2007-07-24 | 2008-04-09 | 汪云华 | Method for preparing manganese sulfate by manganese oxide ore |
| CN101357778A (en) * | 2008-09-24 | 2009-02-04 | 昆明冶金研究院 | Method for producing manganese sulfate by acid leaching under pressure of pyrolusite and pyrite |
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2011
- 2011-06-03 CN CN2011101487209A patent/CN102220491A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157481A (en) * | 2007-07-24 | 2008-04-09 | 汪云华 | Method for preparing manganese sulfate by manganese oxide ore |
| CN101357778A (en) * | 2008-09-24 | 2009-02-04 | 昆明冶金研究院 | Method for producing manganese sulfate by acid leaching under pressure of pyrolusite and pyrite |
Non-Patent Citations (1)
| Title |
|---|
| 《无机盐工业》 20061231 马尧等 "硫酸锰生产新工艺研究" 第39-41页 1-8 第38卷, 第12期 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102605187A (en) * | 2011-10-10 | 2012-07-25 | 云南建水锰矿有限责任公司 | Method for producing manganese sulfate by manganese-rich slag through pressure leaching |
| CN102703698A (en) * | 2012-07-11 | 2012-10-03 | 昆明永瑞防腐有限公司 | Wet metallurgical method for spessartite mineral |
| CN102703698B (en) * | 2012-07-11 | 2014-09-17 | 昆明永新瑞科技有限公司 | Wet metallurgical method for spessartite mineral |
| CN103436696A (en) * | 2013-09-06 | 2013-12-11 | 宁夏天元锰业有限公司 | Method for preparing stock solution for electrolysis to produce metal manganese |
| CN104480314A (en) * | 2014-12-17 | 2015-04-01 | 赵阳臣 | Method for recycling waste residue in manganese industry production |
| CN106756003A (en) * | 2017-01-12 | 2017-05-31 | 江苏凯力克钴业股份有限公司 | The production method that a kind of use potential control is continuously leached |
| WO2024108266A1 (en) * | 2022-11-25 | 2024-05-30 | Element 25 Limited | Process for the recovery of manganese |
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Application publication date: 20111019 |